HRID1889103

反应详情

EQUATION

反应方程式

HRID 1889103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 3-(1,2,4-thiadiazol-5-yl)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine (I115) (30 mg, 0.144 mmol) and triethylamine (0.030 mL, 0.216 mmol) in Dichloromethane (DCM) (2 mL) was stirred at room temperature. 2,4-Dichloro-3-fluorobenzoyl chloride (36.0 mg, 0.158 mmol) in DCM (0.5 ml) was added and stirring continued at room temperature. After 30 mins, 2 drops MeOH were added followed by sat. NaHCO3 solution (3 ml) and ethyl acetate (30 ml). The product was extracted into the ethyl acetate which was dried (Na2SO4) and concentrated. The product was purified by high pH MDAP to give desired product as a white solid after evaporation of the fractions.

WORKUP

后处理

  1. stirringstirring
  2. customcontinued at room temperature
  3. extractionThe product was extracted into the ethyl acetate which
  4. dry with materialwas dried (Na2SO4)
  5. concentrationconcentrated
  6. customThe product was purified by high pH